• Title/Summary/Keyword: X-선 구조분석

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A Study on Dimethacryloyloxy Alkane Derivatives Having an Anti-wear Performance as Lubricating Oil Additives (윤활유첨가제로써 마모억제 성능을 갖는 Dimethacryloyloxy Alkane 유도체에 관한 연구)

  • Han, Hye-Rim;Cho, Jung-Eun;Sim, Dae-Seon;Kang, Chung-Ho;Kim, Young-Wun;Jeong, Noh-Hee;Kang, Ho-Cheol
    • Applied Chemistry for Engineering
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    • v.27 no.6
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    • pp.583-589
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    • 2016
  • Lubricant additives including zinc dialkyldithiophosphate (ZDDP) containing metal have been widely used due to the advantage of very low cost, but they can generate impurities such as ash. In this work, ZDDP containing metals was partially replaced with bis[3-(dialkyloxyphosphorothionyl) thio-2-methylpropanyloxy] butane (BAP4s) which was synthesized conveniently and effectively from alkanediol without any metal components. Also, the wear resistance property of synthesized BAP4s were studied. Wear scar diameter (WSD) values of BAP4s with butyl, octyl, decyl, dodecyl or tetradecyl groups were also measured by four-ball test. As the length of the alkyl group increased from 4 to 8, the WSD value of BAP4s decreased rapidly from 0.59 to 0.45 mm, but from 8 to 14, the value increased very slowly from 0.45 to 0.50 mm. Thus, among all BAP4s, B8P4 having BAP4 with the octyl group, showed the lowest WSD value. Furthermore, the WSD values were measured in a lubricant base oil mixed with a 0.50 percent concentration (w/w) of either BAP4 or ZDDP. The former was 0.55 mm, and the latter was 0.45 mm. The thermal stability and tribofilm formation peroperty were also measured by thermogravimetric analyzer (TGA) and energy-dispersive X-rays spectroscopy (EDS), respectively.

Determination of Crystal Size and Microstrain of $CeO_2$ by Rietveld Structure Refinement (리트벨트 구조분석법에 의한 $CeO_2$의 결정크기 및 미세응력 결정)

  • Hwang, Gil-Chan;Choi, Jin-Beom
    • Journal of the Mineralogical Society of Korea
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    • v.21 no.2
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    • pp.201-208
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    • 2008
  • Ceria ($CeO_2$) becomes one of important functional nanomaterials and a key abrasive material for chemical-mechanical planarization (CMP) of advanced integrated circuits in silicon semi-conductor technology. Two synthetic crystalline ceria (RT735, RT835) are studied by the Rietveld structural refinement to determine crystallite size and microstrain. Rietveld indices of RT735 and RT835 indicate good fitting with $R_p(%)=8.50$, 8.34; $R_{wp}(%)=13.4$, 13.5; $R_{exp}(%)=11.3$, 11.5; $R_B(%)=2.21$, 2.36; S(GofF: Goodness of fit)=1.2, 1.2, respectively. $CeO_2$ with space group Fm3m show a=5.41074(2), 5.41130(6) ${\AA}$, V=158.406(1), 158.455(3)${\AA}^3$ in dimension. Detailed Rietveld refinement reveals that crystallite size and microstrain are 37.42(1) nm, 0.0026 (RT735) and 72.80(2) nm, 0.0013 (RT835), respectively. It also shows that crystallite size and microstrain of ceria are inversely proportional to each other.

Gold Colored Coating of TiO2 thin film on Nickel-Silver by Sol-Gel Process (양백에 코팅된 비정질 TiO2 박막의 특성에 관한 연구)

  • Lim, Yongmu;Kim, Sangmoon;Shim, Moonsik;Jang, Heejin;Shin, Jongyoon;Hwang, Kyuseog
    • Journal of Korean Ophthalmic Optics Society
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    • v.4 no.1
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    • pp.51-56
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    • 1999
  • $TiO_2$ thin films were spin coated on commercial Nickel-Silver with 2%Ti-naphthanate toluene solution by sol-gel process. The thin films were heat-treated at $500^{\circ}C$ for 2min and then decorative-protective coating was obtained. The conditions for gold colored coating, and the morphology, microstructure and color of the coating surface were have been characterized by Optical microscope, Photospectrometer and XRD. The heating temperature of colored-$TiO_2$ coating was $500^{\circ}C$ and was preferable. The average thickness of 1 time coating was $0.24{\mu}m$ and the total thickness increased linearly as a function of the coating time. The color of amorphous colored-$TiO_2$ coating was changed from gold to dark redish gold with coating time. 'L' as lightness and 'b' were decreased to red, but 'a' was decreased to blue after increase with coating time.

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Synthesis and Rietveld Refinement of the Cathode Material $LiFePO_4/C$ for Rechargeable Lithium Batteries (리튬 2차전지용 양극소재 $LiFePO_4/C$의 합성 및 리트벨트 구조분석)

  • Hwang, Gil-Chan;Choi, Jin-Beom;Kim, Jae-Kwang;Ahn, Jou-Hyeon
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.1
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    • pp.63-72
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    • 2009
  • Carbon-coated lithium iron phosphate ($LiFePO_4/C$) composites are synthesized by the modified mechanical activation method (modified MA process) and studied by the Rietveld structural refinement. Rietveld indices of $LiFePO_4/C$ indicate good fitting with $R_p=8.14%,\;R_{wp}=11.1%,\;R_{exp}=9.09%,\;R_B=3.88%$, and S (GofF, Goodness of fit) = 1.2, respectively. $LiFePO_4/C$ with a space group Pnma shows a = 10.3229(3)${\AA}$, b = 6.0052(2) ${\AA}$, c = 4.6939(1) ${\AA}$, and V = 290.98(1) ${\AA}^3$ in dimension, indicating good agreements with those of previous works. Synthetic powders are nano-sized ($65{\sim}90nm$) homogeneous particles with high purity. Thus the modified MA method will be an efficient process to get a high quality cathode material for commercial lithium batteries.

Characterization on the Behavior of Heavy Metals and Arsenic in the Weathered Tailings of Songcheon Mine (송천광산의 풍화광미 내 중금속 및 비소 거동 특성)

  • Lee, Woo-Chun;Kim, Young-Ho;Cho, Hyen-Goo;Kim, Soon-Oh
    • Journal of the Mineralogical Society of Korea
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    • v.23 no.2
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    • pp.125-139
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    • 2010
  • Behavior of heavy metals and arsenic in the tailings of Songcheon Au-Ag mine was characterized via both mineralogical and geochemical methods. Mineral composition of the tailings was investigated by X-ray diffractometry, energy-dispersive spectroscopy, and electron probe micro-analyzer (EPMA) and total concentrations of heavy metals and arsenic and their chemical forms were analyzed by total digestion of aqua regia and sequential extraction method, respectively. The results of mineralogical study indicate that the tailings included mineral particles of resinous shape mainly consisting of galena, sphalerite, pyrite, quartz, and scorodite, and specifically socordite was identified in the form of matrix. EPMA quantitative analyses were performed to evaluate the weatherability of each mineral, and the results suggest that it decreased in the sequence of arsenopyrite > galena > sphalerite > pyrite. The weathering pattern of galena was observed to show distinctive zonal structure consisting of secondary minerals such as anglesite and beudantite. In addition, almost all of arsenopyrite has been altered to scorodite existing asmatrix and galena, sphalerite, and pyrite which have lower weatherability than arsenopyrite were identified within the matrix of scorodite. During the process of alteration of arsenopyrite into scorodite, it is likely that a portion of arsenic was lixiviated and caused a great deal of detrimental effects to surrounding environment. The results of EPMA quantitative analyses verify that the stability of scorodite was relatively high and this stable scorodite has restrained the weathering of other primary minerals within tailings as a result of its coating of mineral surfaces. For this reason, Songcheon tailings show the characteristics of the first weathering stage, although they have been exposed to the surface environment for a long time. Based on the overall results of mineralogical and geochemical studies undertaken in this research, if the tailings are kept to be exposed to the surface environment and the weathering process is continuous, not only hazardous heavy metals, such as lead and arsenic seem to be significantly leached out because their larger portions are being partitioned in weakly-bound (highly-mobile) fractions, but the potential of arsenic leaching is likely to be high as the stability of scorodite is gradually decreased. Consequently, it is speculated that the environmental hazard of Songcheon mine is significantly high.

Phase Transformation of 2 Components(CaO-, $Y_2O_3$-, MgO-$ZrO_2$) and 3 Components(MgO-$ZrO_2-Al_2O_3)$ Zirconia by X-ray Diffraction and Raman Spectroscopy (X-선회절과 Raman 분광분석을 이용한 2성분계(CaO-, $Y_2O_3$-, MgO-$ZrO_2$) 및 3성분계(MgO-$ZrO_2-Al_2O_3)$ Zirconia의 상전이연구)

  • 은희태;황진명
    • Journal of the Korean Ceramic Society
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    • v.34 no.2
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    • pp.145-156
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    • 1997
  • ZrO2 phase transformations depending on the type and amount of dopants and the sintering temperatures were studied for the 2 components (CaO-, Y2O3-, MgO-ZrO2) and the 3 components(MgO-ZrO2-Al2O3)ZrO2 powder by X-ray diffraction and Raman spectroscopy. In the CaO- and Y2O3-ZrO2 systems, as the CaO and Y2O3 contents increased to 6~15mol% and 3~15mol% respectively, we were not able to identify between tetragonal and cubic in the X-ray diffraction patterns. On the other hand, all Raman modes shifted to lower wavenumbers, decreasing in intensity and the number of bands, markedly. These phenomena were caused by tetragonallongrightarrowcubic phase transformation and interpreted by the breakdown of the wave vector selection rule(k=0) and the structural disorder associated with the formation of oxygen sublattice which was caused by the substitution between Zr4+ ion and Ca2+ or Y3+ ion in ZrO2 matrix. The monoclinic to cubic phase transformation occurred in 10mol% MgO-ZrO2 system. As the Al2O3 content increased from 0 to 20mol% in the MgO-ZrO2-Al2O3 systems, cubic phase transformed to monoclinic phase, this is because the MgO didn't play a role in a stabilizer because of the formation of the spinel(MgAl2O4) by the reaction between MgO and Al2O3, Also, the ZrO2 phase transformation was explained by the change of it's lattice parameters depending on the type and amount of dopants. Namely, as the amount of dopant increased to 10~13mol%, the axial ra-tio c/a came close to unity with increasing the lattice parameter a and decreasing the lattice parameter c. At that time, the tetragonallongrightarrowcubic phase transformation occurred.

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Effects of SiO2 Incorporation on Catalytic Performance and Physico-Chemical Properties of Iron-Based Catalysts for the Fischer-Tropsch Synthesis (Fischer-Tropsch 합성반응용 Fe계 촉매의 성능 및 물리화학적 특성에 미치는 SiO2 첨가효과)

  • Hyun, Sun-Taek;Chun, Dong Hyun;Kim, Hak-Joo;Yang, Jung Hoon;Yang, Jung-Il;Lee, Ho-Tae;Lee, Kwan-Young;Jung, Heon
    • Korean Chemical Engineering Research
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    • v.48 no.3
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    • pp.304-310
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    • 2010
  • The FTS(Fischer-Tropsch synthesis) was carried out over precipitated iron-based catalysts with or without $SiO_2$ in a fixed-bed reactor at $250^{\circ}C$ and 1.5 MPa. The catalysts with $SiO_2$ showed much higher catalytic activity for the FTS than those without $SiO_2$, displaying excellent stability during 144 h of reaction. The X-ray diffraction and $N_2$ physisorption revealed that the catalysts with $SiO_2$ showed enhanced dispersion of $Fe_2O_3$ compared with those without $SiO_2$. Also, the results of temperature-programmed reduction by $H_2$ showed that the addition of $SiO_2$ markedly promoted the reduction of $Fe_2O_3$ into $Fe_3O_4$ and FeO at low temperatures below $260^{\circ}C$. In contrast, surface basicity of the catalysts, which was analyzed by temperature-programmed desorption of $CO_2$, decreased as a result of $SiO_2$ addition. We attribute the high and stable performance of the catalysts with $SiO_2$ to the improved dispersion and reducibility by the $SiO_2$ addition.

A study on the production techniques and prototype of the mother-of-pearl chrysanthemum pattern box from the Goryeo Dynasty (고려 나전국화넝쿨무늬상자의 제작기법 고찰 및 원형 연구)

  • LEE Heeseung;LEE Minhye;KIM Sunghun;LEE Hyeonju
    • Korean Journal of Heritage: History & Science
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    • v.57 no.1
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    • pp.126-144
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    • 2024
  • The chrysanthemum vine pattern box from the Goryeo Dynasty expresses in great detail the representative features of Goryeo Dynasty lacquerware with mother-of-pearl, such as engraving patterns on the surface of fine mother-of-pearl, expressing vine stems using metal wires, and twisting metal wires to form the boundaries of each patterns. While the lacquerware with mother-of-pearl that remains today from the Goryeo Dynasty has the form of a sutra box and a box with lid, the chrysanthemum vine pattern box that is the subject of this study is in the shape of a box with a separate lid and body, making it difficult to estimate the purpose of production or the stored contents. In this study, we attempted to confirm the formative characteristics of the chrysanthemum vine pattern box in order to confirm its original form, and to investigate its structure and production technique through X-ray transmission. In addition, we attempted to identify the use and production purpose of the box by classifying and comparing the previously known lacquerware with mother-ofpearl from the Goryeo Dynasty by type. As a result of the investigation, fabric was confirmed the bottom of body and inner box through X-ray images. Through this, it was confirmed that the 'Mogsimjeopichilgi'(wooden core grabbing fabric technique) of wrapping the object with fabric was used. And through wood grain, it was possible to confirm the wooden board composition of the part presumed to be the restored part and the part presumed to have had existing Jangseog. In addition, it was confirmed that the joints were connected in a Majdaeim(part to part). Based on the survey results, a total of 14 pieces, including 9 Sutra boxes, 3 boxes, and 2 small boxes, that remain from the Goryeo Dynasty were classified by type and examined for similarity. Among them, there is a "Chrysanthemum Vine Pattern Sutra Box" from a private collection in Japan, a "Black Lacquered Chrysanthemum Arabesque Bun Sutra Box" from the Tokugawa Art Museum, a "Sutra Holder" from the British Museum, and a "Small Box with a Mother-of-Pearl Chrysanthemum Vine Pattern" from a private collection in Korea. The pattern composition of five points was most similar to the subject of this study. As a result of comparing the damage pattern, formative characteristics, and structural features of each part, it is presumed that the sutra holder in the British Museum was transformed into its current form from the original the chrysanthemum vine patterned box. Lastly, in order to confirm the purpose of production, that is, the use of this box, we investigated examples of Tripitaka Koreana printed version produced at a time similar to the social atmosphere of Goryeo at the time. Following the Mongol(元) invasion after the Goryeo military regime at the time, sutras appeared to pray for the stability of the nation and the soul of an individual, and with the development of domestic printing and paper in the 13th century, it gradually coincided with the transition from a scroll to a folded form, and the form of a box changed from a box. It is believed that the storage method also changed.

High-temperature Thermal Decomposition of Cs-adsorbed CHA-Cs and CHA-PCFC-Cs Zeolite System, and Sr-adsorbed 4A-Sr and BaA-Sr Zeolite System (Cs-흡착 CHA-Cs 및 CHA-PCFC-Cs 제올라이트계와 Sr-흡착 4A-Sr 및 BaA-Sr 제올라이트계의 고온 열분해)

  • Lee, Eil-Hee;Kim, Ji-Min;Kim, Hyung-Ju;Kim, Ik-Soo;Chung, Dong-Yong;Kim, Kwang-Wook;Lee, Keun-Young;Seo, Bum-Kyoung
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.16 no.1
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    • pp.49-58
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    • 2018
  • For the immobilization of high-radioactive nuclides such as Cs and Sr by high-temperature thermal decomposition, this study was carried out to investigate the phase transformation with calcined temperature by using TGA (thermogravimetric analysis) and XRD (X-ray diffraction) in the Cs-adsorbed CHA (chabazite zeolite of K type)-Cs and CHA-PCFC (potassium cobalt ferrocyanide)-Cs zeolite system, and Sr-adsorbed 4A-Sr and BaA-Sr zeolite system, respectively. In the case of CHA-Cs zeolite system, the structure of CHA-Cs remained at up to $900^{\circ}C$ and recrystallized to pollucite ($CsAlSi_2O_6$) at $1,100^{\circ}C$ after undergoing amorphous phase at $1,000^{\circ}C$. However, the CHA-CFC-Cs zeolite system retained the CHA-PCFC-Cs structure up to $700^{\circ}C$, but its structure collapsed in $900{\sim}1,000^{\circ}C$, and then transformed to amorphous phase, and recrystallized to pollucite at $1,100^{\circ}C$. In the case of 4A-Sr zeolite system, on the other hand, the structure of 4A-Sr maintained up to $700^{\circ}C$ and its phase transformed to amorphous at $800^{\circ}C$, and recrystallized to Sr-feldspar ($SrAl_2Si_2O_8$, hexagonal) at $900^{\circ}C$ and to $SrAl_2Si_2O_8$ (triclinic) at $1,100^{\circ}C$. However, the BaA-Sr zeolite system structure began to break down at below $500^{\circ}C$, and then transformed to amorphous phase in $500{\sim}900^{\circ}C$ and recrystallized to Ba/Sr-feldspar (coexistence of $Ba_{0.9}Sr_{0.1}Al_2Si_2O_8$ and $Ba_{0.5}Sr_{0.5}Al_2Si_2O_8$) at $1,100^{\circ}C$. All of the above zeolite systems recrystallized to mineral phase through the dehydration/(decomposition) ${\rightarrow}$ amorphous ${\rightarrow}$ recrystallization with increasing temperature. Although further study of the volatility and leachability of Cs and Sr in the high-temperature thermal decomposition process is required, Cs and Sr adsorbed in each zeolite system are mineralized as pollucite, Sr-feldspar and Ba/Sr-feldspar. Therefore, Cs and Sr seen to be able to completely immobilize in the calcining wasteform/(solidified wasteform).

Si 함유 다이아몬드상 카본 필름의 환경 변화에 따른 마찰거동 연구

  • 박세준;이광렬;공호성;양승호
    • Proceedings of the Korean Vacuum Society Conference
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    • 2000.02a
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    • pp.126-126
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    • 2000
  • 다이아몬드상 카본(DLC) 필름은 경도가 높고, 마찰계수가 낮다는 장점을 가지고 있기 때문에 내마모성 코팅이나 윤활성코팅에 응용을 위한 연구가 활발히 진행중이다. 하지만 마찰계수가 주변환경에 매우 큰 영향을 받는다는 단점이 있다. 이러한 단점은 DLC필름의 응용에 대한 저해 요인이 되며, 이 점을 보완하기 위해서 DLC 필름에 Si을 첨가하는 연구들이 진행되고 있다. 본 실험에서는 r.f-PACVD 법을 이용하여 Si이 첨가된 DLC 필름의 주위 환경 변화에 따른 마찰특성의 변화를 연구하였다. 사용한 반응 가스는 벤젠(C6H)과 희석된 Silane(SiH4 : H2 = 10 : 90)이며, 희석된 Silane과 벤젠의 첨가비율을 조절하여 필름내 Si의 함량을 조절하였고, 증착시 바이아스의 전압은 -400V로 하였다. 마찰테스트는 Ball-on-Disk type의 조건에서 대기, 건조공기, 진공의 세가지 분위기에서 마찰테스트를 실행하였다. 실험결과 마찰계수는 건조공기, 대기, 진공의 순으로 증가하였고, 필름내에 포함되어 있는 Si의 양이 증가할수록 마찰계수는 낮고 안정한 값을 나타내었다. Tribochemiacal 분석과, ball과 track의 전자현미경 사진 분석 결과, 진공에 비해서 건조공기와 대기중에서 마찰계수가 낮은 것은 DLC 필름내에 마모 track 중심부에 Si-C-O 계의 화합물이 형성되어, 이 화합물이 마찰계면에 존재하여 마찰계수를 낮추었음을 확인하였다. 그리고 대기중에서 실험한 경우, 습기의 존재로 인해 마모입자가 볼의 표면에서 엉김으로써 건조공기의 상태에서 보다 높은 마찰저항을 갖게 됨으로 인하여 마찰계수가 높아짐을 알 수 있었다.a)는 as-deposit 상태이며, 그림 1(b)는 45$0^{\circ}C$, 60min 열처리한 plan-view TEM 사진이다.dical의 영향을 조사하였으며 oxygen radical의 rf power에 따른 변화는 OES(Optical emission spectroscopy)를 사용하였다. 너무 적은 oxygen ion beam flux나 oxygen radical은 film의 전도도 및 투과도를 저하시켰고 반면 너무 과도한 flux의 증가 시는 전도도는 감소하였고 투과도는 증가하는 경향을 보였다. 기판에 도달하는 oxygen ion flux는 faraday cup을 이용하여 측정하였으며 증착된 ITO film은 XPS, UV-spectrometer, 4-point probe를 이용하여 분석하였다. 때문으로 생각되어진다. 또한, 성장 온도가 낮아짐에 따라 AlGaN의 성장을 저해하기 때문으로 판단된다. 성장 온도 변화에 따라 성장된 V의 구조적 특성 및 표면 거칠기 변화를 관찰하여 AlGaN의 성장 거동을 논의하겠다.034, 0.005 정도로 다시 감소하였다. 박막의 유전율은 약 35 정도의 값을 나타내었으며 X-선 회절 data로부터 분석한 박막의 변형은 증온도에 따라 7.2%에서 0.04%로 감소하였고 이 이경향은 유전손실은 감소경향과 일치하였다.는 현저하게 향상되었다. 그 원인은 SB power의 인가에 의해 활성화된 precursor 분자들이 큰 에너지를 가지고 기판에 유입되어 치밀한 박막이 형성되었기 때문으로 사료된다.을수 있었다.보았다.다.다양한 기능을 가진 신소재 제조에 있다. 또한 경제적인 측면에서도 고부가 가치의 제품

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